WO2010084922A1 - Glass for scattering layer of organic led device and organic led device - Google Patents
Glass for scattering layer of organic led device and organic led device Download PDFInfo
- Publication number
- WO2010084922A1 WO2010084922A1 PCT/JP2010/050727 JP2010050727W WO2010084922A1 WO 2010084922 A1 WO2010084922 A1 WO 2010084922A1 JP 2010050727 W JP2010050727 W JP 2010050727W WO 2010084922 A1 WO2010084922 A1 WO 2010084922A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- glass
- organic led
- scattering layer
- layer
- led element
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
- C03C17/04—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass by fritting glass powder
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/21—Silica-free oxide glass compositions containing phosphorus containing titanium, zirconium, vanadium, tungsten or molybdenum
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
- C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
- C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/02—Details
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/48—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific function
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/80—Constructional details
- H10K50/85—Arrangements for extracting light from the devices
- H10K50/854—Arrangements for extracting light from the devices comprising scattering means
Definitions
- the present invention relates to glass, particularly glass used for a scattering layer of an organic LED element, and an organic LED element using the glass.
- the organic LED element has an organic layer. And there exists a bottom emission type which takes out the light produced
- Patent Document 1 has a problem that the content of the glass composition is not disclosed or suggested, and cannot be implemented.
- the scattering layer glass of the organic LED element of one embodiment of the present invention is expressed in terms of mol% based on oxide, P 2 O 5 : 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27% and ZnO: 15 to 35%, and the total content of alkali metal oxides composed of Li 2 O, Na 2 O, and K 2 O is 5% by mass or less It is characterized by that.
- An organic LED element of one embodiment of the present invention includes a transparent substrate, a first electrode provided on the transparent substrate, an organic layer provided on the first electrode, and a second electrode provided on the organic layer.
- P 2 O 5 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27%, ZnO: 10 It is characterized by having a scattering layer containing ⁇ 35% and containing a total amount of alkali metal oxides composed of Li 2 O, Na 2 O and K 2 O of 5% by mass or less.
- the present invention it is possible to provide a glass of a scattering layer used for an organic LED element or an organic LED element using the scattering layer.
- Sectional drawing of the 1st organic LED element of this invention Sectional drawing of the 2nd organic LED element of this invention Graph showing the relationship between the refractive index of ITO and the refractive index of glass for scattering layer
- Top view showing the structure of a device having a scattering layer
- Top view showing the structure of an element without a scattering layer
- Graph showing the relationship between voltage and current Graph showing the relationship between luminous flux and current
- Conceptual diagram of a system for evaluating the angular dependence of light emission Graph showing the relationship between brightness and angle Graph showing the relationship between chromaticity and angle
- FIG. 1 is a cross-sectional view of a first organic LED element of the present invention.
- the first organic LED element of the present invention is a bottom emission type organic LED element.
- the first organic LED element of the present invention includes a transparent substrate 110, a scattering layer 120 formed on the transparent substrate 110, a first electrode 130 formed on the scattering layer 120, and the first electrode 130.
- the organic layer 140 is formed on the organic layer 140, and the second electrode 150 is formed on the organic layer 140.
- the first electrode 130 is a transparent electrode (anode)
- the second electrode 150 is a reflective electrode (cathode).
- the first electrode 130 has transparency for transmitting light emitted from the organic layer 140 to the scattering layer 120.
- the second electrode 150 has reflectivity for reflecting light emitted from the organic layer 140 and returning it to the organic layer 140.
- FIG. 2 is a cross-sectional view of the second organic LED element of the present invention.
- the second organic LED element of the present invention is a double-sided emission type organic LED element.
- the second organic LED element of the present invention includes a transparent substrate 110, a scattering layer 120 formed on the transparent substrate 110, a first electrode 130 formed on the scattering layer 120, and the first electrode 130.
- the organic layer 140 is formed on the organic layer 140, and the second electrode 210 is formed on the organic layer 140.
- the first electrode 130 is a transparent electrode (anode)
- the second electrode 210 is a transparent electrode (cathode).
- the first electrode 130 has transparency for transmitting light emitted from the organic layer 140 to the transparent substrate 110.
- the second electrode 210 has transparency for transmitting light emitted from the organic layer 140 to a surface opposite to the surface facing the organic layer 140.
- This organic LED element is used as an illumination application in which light is emitted from the front and back surfaces.
- a material having a high visible light transmittance As the light-transmitting substrate used for forming the transparent substrate 110, a material having a high visible light transmittance, such as a glass substrate, is mainly used. Specifically, a material having a high transmittance is a plastic substrate in addition to a glass substrate. Examples of the material of the glass substrate include inorganic glass such as alkali glass, non-alkali glass, and quartz glass. In order to prevent the diffusion of the glass component, a silica film or the like may be coated on the surface of the glass substrate.
- the plastic substrate material examples include polyester, polycarbonate, polyether, polysulfone, polyethersulfone, polyvinyl alcohol, and fluorine-containing polymers such as polyvinylidene fluoride and polyvinyl fluoride.
- the plastic substrate may have a barrier property.
- the thickness of the transparent substrate is preferably 0.1 mm to 2.0 mm in the case of glass. However, if the thickness is too thin, the strength decreases, so that the thickness is particularly preferably 0.5 mm to 1.0 mm.
- the scattering layer 120 is formed by forming glass powder on a substrate by a method such as coating and baking at a desired temperature, and is dispersed in the base material 121 having the first refractive index and the base material 121. And a plurality of scattering materials 122 having a second refractive index different from that of the base material 121. In the plurality of scattering materials 122, the distribution of the scattering materials in the scattering layer is reduced from the inside of the scattering layer to the outermost surface.
- the scattering layer is made of glass, so that it has excellent scattering characteristics while maintaining the smoothness of the surface. By using it on the light-emitting surface side of light-emitting devices, extremely efficient light extraction is possible. Can be realized.
- the scattering layer glass (base material) having a high light transmittance is used.
- a plurality of scattering substances for example, bubbles, precipitated crystals, material particles different from the base material, and phase-separated glass
- the particle refers to a small solid substance such as a filler or ceramic.
- Air bubbles refer to air or gas objects.
- phase-separated glass means the glass comprised by two or more types of glass phases.
- the refractive index of the base material is preferably equal to or higher than the refractive index of the first electrode. This is because when the refractive index is low, a loss due to total reflection occurs at the interface between the base material and the first electrode.
- the refractive index of the base material only needs to exceed at least a part of the emission spectrum range of the organic layer (for example, red, blue, green, etc.), but exceeds the entire emission spectrum range (430 nm to 650 nm). It is more preferable that it exceeds the entire wavelength range of visible light (360 nm to 830 nm).
- the refractive index of the first electrode may be higher than the refractive index of the base material as long as the difference between the refractive index of the base material and the refractive index of the first electrode is within 0.2.
- the main surface of the scattering layer needs to be smooth.
- the scattering material protrudes from the main surface of the scattering layer.
- the scattering material does not protrude from the main surface of the scattering layer, it is preferable that the scattering material does not exist within 0.2 ⁇ m from the main surface of the scattering layer.
- the arithmetic average roughness (Ra) defined in JIS B0601-1994 of the main surface of the scattering layer is preferably 30 nm or less, more preferably 10 nm or less (see Table 1), and particularly preferably 1 nm or less.
- Both the scattering material and the base material may have a high refractive index, but the difference in refractive index ( ⁇ n) is preferably 0.2 or more in at least a part of the emission spectrum range of the light emitting layer. In order to obtain sufficient scattering characteristics, the difference in refractive index ( ⁇ n) is 0.2 or more over the entire emission spectrum range (430 nm to 650 nm) or the entire visible light wavelength range (360 nm to 830 nm). More preferred.
- the base material has a high refractive index glass and the scattering material has a gaseous object, that is, a bubble.
- the colorant known ones such as transition metal oxides, rare earth metal oxides and metal colloids can be used alone or in combination.
- Whitening is a method of spatially painting red, blue, and green (painting method), a method of laminating light emitting layers having different emission colors (lamination method), and providing blue light that is separated spatially.
- a method (color conversion method) for performing color conversion with a color conversion material is known.
- a white layer can be obtained uniformly, so a lamination method is common.
- the light emitting layer to be stacked uses a combination that turns white by additive color mixing.
- a blue-green layer and an orange layer may be stacked, or red, blue, and green may be stacked.
- color reproducibility on the irradiated surface is important, and it is desirable to have a necessary emission spectrum in the visible light region.
- the blue-green layer and the orange layer are laminated, the green light emission intensity is low, and therefore, when a light containing a lot of green is illuminated, the color reproducibility is deteriorated.
- the lamination method has an advantage that it is not necessary to spatially change the color arrangement, it has the following two problems.
- the first problem is that since the organic layer is thin, the extracted emitted light is affected by interference. Therefore, the color changes depending on the viewing angle. In the case of white, such a phenomenon may be a problem because the sensitivity to the color of human eyes is high.
- the second problem is that the carrier balance is shifted while the light is emitted, the light emission luminance of each color is changed, and the color is changed.
- a fluorescent material can be used as a scattering material or a base material. Therefore, the effect of changing the color by performing wavelength conversion can be brought about by the light emission from the organic layer. In this case, the light emission color of the organic LED can be reduced, and the emitted light is scattered and emitted, so that the angle dependency of the color and the temporal change of the color can be suppressed.
- the first electrode is required to have a translucency of 80% or more in order to extract light generated in the organic layer 140 to the outside.
- a high work function is required to inject many holes.
- ITO Indium Tin Oxide
- SnO 2 , ZnO, IZO Indium Zinc Oxide
- AZO ZnO—Al 2 O 3 : zinc oxide doped with aluminum
- GZO ZnO—Ga 2 O 3 : zinc oxide doped with gallium
- Nb-doped TiO 2 , Ta-doped TiO 2 and other materials are used.
- the thickness of the anode is preferably 100 nm or more.
- the refractive index of the anode 130 is 1.9 to 2.2.
- the refractive index of ITO can be lowered.
- SnO 2 has a standard of 10 wt%. From this, the refractive index of ITO can be lowered by increasing the Sn concentration.
- the carrier concentration increases as the Sn concentration increases, there is a decrease in mobility and transmittance. Therefore, it is necessary to determine the amount of Sn by balancing these.
- the first electrode used mainly in the bottom emission type organic LED element has been described, but it goes without saying that the first electrode may be used in a double-sided light emitting type organic LED element.
- the organic layer 140 is a layer having a light emitting function, and includes a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, and an electron injection layer.
- the refractive index of the organic layer 140 is 1.7 to 1.8.
- the hole injection layer is required to have a small difference in ionization potential in order to lower the hole injection barrier from the anode. Improvement of the charge injection efficiency from the electrode interface in the hole injection layer lowers the drive voltage of the device and increases the charge injection efficiency.
- PEDOT Polyethylene dioxythiophene
- PSS polystyrene sulfonic acid
- CuPc phthalocyanine-based copper phthalocyanine
- the hole transport layer serves to transport holes injected from the hole injection layer to the light emitting layer. It is necessary to have an appropriate ionization potential and hole mobility.
- the hole transport layer may be a triphenylamine derivative, N, N′-bis (1-naphthyl) -N, N′-diphenyl-1,1′-biphenyl-4,4′-diamine (NPD ), N, N′-diphenyl-N, N′-bis [N-phenyl-N- (2-naphthyl) -4′-aminobiphenyl-4-yl] -1,1′-biphenyl-4,4 ′ -Diamine (NPTE), 1,1-bis [(di-4-tolylamino) phenyl] cyclohexane (HTM2) and N, N'-diphenyl-N, N'-bis (3-methylphenyl) -1,1 '-Diphenyl-4,4'-diamine (TPD) or the like is used.
- the thickness of the hole transport layer is preferably 10 nm to 150 nm. The thinner the thickness is, the
- the light emitting layer uses a material that provides a field where injected electrons and holes recombine and has high luminous efficiency. More specifically, the light emitting host material and the light emitting dye doping material used in the light emitting layer function as recombination centers of holes and electrons injected from the anode and the cathode, and light emission to the host material in the light emitting layer The doping of the dye obtains high luminous efficiency and converts the emission wavelength. These are required to have an appropriate energy level for charge injection, to form a uniform amorphous thin film having excellent chemical stability and heat resistance.
- Light emitting materials that are organic materials include low-molecular materials and high-molecular materials. Further, it is classified into a fluorescent material and a phosphorescent material according to the light emission mechanism.
- the light-emitting layer includes tris (8-quinolinolato) aluminum complex (Alq 3 ), bis (8-hydroxy) quinaldine aluminum phenoxide (Alq ′ 2 OPh), bis (8-hydroxy) quinaldine aluminum— 2,5-dimethylphenoxide (BAlq), mono (2,2,6,6-tetramethyl-3,5-heptanedionate) lithium complex (Liq), mono (8-quinolinolato) sodium complex (Naq), Mono (2,2,6,6-tetramethyl-3,5-heptanedionate) lithium complex, mono (2,2,6,6-tetramethyl-3,5-heptanedionate) sodium complex and bis ( 8-quinolinolato) calcium complex (CAQ 2) metal complexes of quinoline derivatives such as tetraphenyl butadiene, off Nirukinakudorin (QD), anthracene, and a fluorescent substance such as perylene and coronene
- the electron transport layer serves to transport electrons injected from the electrode.
- the electron transport layer is formed of a quinolinol aluminum complex (Alq 3 ), an oxadiazole derivative (for example, 2,5-bis (1-naphthyl) -1,3,4-oxadiazole (BND) and 2 -(4-t-butylphenyl) -5- (4-biphenyl) -1,3,4-oxadiazole (PBD) and the like), triazole derivatives, bathophenanthroline derivatives, silole derivatives and the like are used.
- the electron injection layer is required to increase the electron injection efficiency.
- the electron injection layer is provided with a layer doped with an alkali metal such as lithium (Li) or cesium (Cs) at the cathode interface.
- a metal having a small work function or an alloy thereof is used.
- the cathode include alkali metals, alkaline earth metals, metals of Group 3 of the periodic table, and the like.
- aluminum (Al), magnesium (Mg), silver (Ag), or alloys thereof are preferably used because they are inexpensive and have good chemical stability.
- a laminated electrode in which Al is vapor-deposited on a co-deposited film of Al, MgAg, a thin film deposited film of LiF or Li 2 O, or the like is used.
- the reflective electrode may be used as an anode.
- the second electrode when used in the second organic LED element of the double-sided emission type, it is not reflective but requires translucency. Therefore, the configuration and characteristics at that time are preferably the same as those of the first electrode.
- the scattering layer glass of the organic LED element of the present invention will be described in detail. Since the refractive index of the glass for a scattering layer is preferably equal to or higher than the refractive index of the translucent electrode material as described above, it is desirable that it be as high as possible.
- the glass transition temperature of the glass for the scattering layer is desirably as low as possible in order to prevent thermal deformation of the substrate when the glass powder is fired and softened to form the scattering layer.
- the thermal expansion coefficient of the glass for the scattering layer must be close to or slightly lower than the thermal expansion coefficient of the substrate in order to prevent the phenomenon of cracking or warping due to stress generated between the scattering layer and the substrate. There is.
- the glass having a high refractive index and a low transition temperature has a coefficient of thermal expansion that is much larger than the coefficient of thermal expansion of the substrate. Therefore, it is desirable that the coefficient of thermal expansion of the glass for the scattering layer be as low as possible. Warpage and cracking become a major obstacle when forming a translucent electrode layer on a scattering layer.
- P 2 O 5 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27%, ZnO: 10 to 35 %, And the total content of alkali metal oxides composed of Li 2 O, Na 2 O, and K 2 O is 5% by mass or less.
- P 2 O 5 is a component that forms a network structure serving as a skeleton of the glass and stabilizes the glass, and is essential. When P 2 O 5 is less than 15 mol%, devitrification is likely to occur. 19 mol% or more is preferable, and 20 mol% or more is more preferable.
- Bi 2 O 3 is a component that imparts a high refractive index and increases the stability of the glass, and is essential. If it is less than 5%, the effect becomes insufficient. 10 mol% or more is preferable and 13 mol% or more is more preferable. On the other hand, when it exceeds 25 mol%, the thermal expansion coefficient is increased, and the coloring is easily increased. 23 mol% or less is preferable and 20 mol% or less is more preferable.
- Nb 2 O 5 is a component that imparts a high refractive index and lowers the thermal expansion coefficient, and is essential. If it is less than 5 mol%, the effect becomes insufficient. 7 mol% or more is preferable and 10 mol% or more is more preferable. On the other hand, when it exceeds 27 mol%, the glass transition temperature is increased and devitrification is likely to occur. 20 mol% or less is preferable and 18 mol% or less is more preferable.
- ZnO is a component that greatly lowers the glass transition temperature and increases the refractive index while suppressing an excessive increase in the thermal expansion coefficient, and is essential. If it is less than 10 mol%, the effect becomes insufficient.
- 16 mol% or more is preferable and 18 mol% or more is more preferable.
- it exceeds 35 mol% the devitrification tendency of the glass increases.
- 30 mol% or less is preferable and 27 mol% or less is more preferable.
- correspond one-to-one with mol% notation when expressed in mass%, 7 mass% or more is preferable.
- Alkali metal oxides composed of Li 2 O, Na 2 O and K 2 O may increase the thermal expansion coefficient. Therefore, it is preferable not to contain substantially (content is substantially zero). However, since it has the effect of giving the glass devitrification resistance and lowering the glass transition temperature, it may be contained up to 7 mol%.
- the alkali metal may move when an electric field is applied in a humid state, and may destroy the terminal of the organic LED element. Therefore, the total amount of the alkali metal oxide is preferably 5% by mass or less, more preferably 2% by mass or less, and particularly preferably substantially not contained (the content is substantially zero).
- Na 2 O and K 2 O since the result in particularly large thermal expansion coefficient compared to Li 2 O, if the inclusion of alkali metal oxides, substantially free of Na 2 O and K 2 O (Content is almost zero), it is preferable to use only Li 2 O. TiO 2 tends to devitrify as the glass transition temperature rises. Therefore, it is preferable that TiO 2 is not substantially contained (the content is substantially zero).
- B 2 O 3 is not essential, but has an effect of improving the solubility of the glass. Therefore, you may contain to 17 mol%. However, if it exceeds 17 mol%, devitrification and phase separation are likely to occur, and it becomes difficult to obtain a high refractive index.
- WO 3 is not essential, but has the effect of imparting a high refractive index without significantly changing the thermal expansion coefficient and glass transition temperature. Therefore, you may contain to 20 mol%. However, when it exceeds 20 mol%, coloring increases and devitrification easily occurs.
- TeO 2 is not essential, but has an effect of lowering the glass transition temperature while suppressing an excessive increase in the thermal expansion coefficient. Therefore, you may contain to 7 mol%. However, it is expensive and may erode the platinum crucible, so it is preferable not to use a large amount.
- GeO 2 is not essential, but has an effect of imparting a high refractive index. Therefore, you may contain to 7 mol%. However, since it is expensive, it is preferable not to use a large amount.
- Sb 2 O 3 is not essential, but it is not only effective as a clarifying agent but also has an effect of suppressing coloring. Therefore, you may contain to 2 mol%.
- Alkaline earth metal oxides (MgO, CaO, SrO, BaO) are not essential, but have the effect of improving the stability of the glass. Therefore, you may contain to 10 mol%. However, if the content exceeds 10 mol%, the refractive index is lowered and the thermal expansion coefficient is increased. In addition, it does not contain substantially when it does not contain substantially, and includes the case where it mixes as an impurity by other ingredients origin.
- the glass of the present invention is SiO 2 , Al 2 O 3 , La 2 O 3 , Y 2 O 3 , Gd 2 O 3 , ZrO 2 , Ta 2 O 3 , Cs 2 O, as long as the effects of the invention are not lost. Transition metal oxides and the like can also be contained. Their total content is preferably less than 5 mol%, more preferably less than 3 mol%, and particularly preferably substantially no content (the content is almost zero). In addition, since the glass of this invention does not contain lead oxide substantially, possibility of causing environmental pollution is low.
- the glass of the present invention uses raw materials such as oxides, phosphates, metaphosphates, carbonates, nitrates, and hydroxides, weighs them so as to have a predetermined composition, mixes them, platinum, etc. It can be obtained by melting at a temperature of 950 to 1500 ° C. using a crucible and casting into a mold or pouring into a gap between twin rolls and quenching. Also, it may be gradually cooled to remove the distortion.
- the glass produced by the above method is used in the form of powder.
- the glass powder is obtained by pulverizing glass with a mortar, ball mill, jet mill or the like, and classifying it as necessary.
- the mass average particle size of the glass powder is typically 0.5 to 10 microns.
- the surface of the glass powder may be modified with a surfactant or a silane coupling agent.
- This glass frit is kneaded with a solvent or a binder as necessary, and then applied onto a transparent substrate and fired at a temperature about 60 ° C. higher than the glass transition temperature of the glass frit to soften the glass frit and cool to room temperature. By doing so, a transparent substrate with a scattering layer is obtained.
- the solvent examples include ⁇ -terpineol, butyl carbitol acetate, phthalate ester, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate
- the binder includes ethyl cellulose, acrylic resin, styrene resin, Examples thereof include phenol resin and butyral resin.
- Tables 1 to 3 show the composition of the glass expressed in mol% in each example, the refractive index (n d ), the glass transition temperature (T g ), and the average thermal expansion coefficient from 50 ° C. to 300 ° C. ( ⁇ 50-300 ).
- the composition in terms of mass% converted based on the composition in terms of mol% is also shown.
- oxides, metaphosphates or carbonates are used as raw materials for each component. After vitrification, the raw materials are weighed so as to have the composition shown in Table 1 and mixed sufficiently, and then a platinum crucible is used. After melting in a temperature range of 950 ° C. to 1350 ° C.
- the refractive index (n d ) After the glass was polished, it was measured by a V-block method using a Kalun precision refractometer KPR-2000.
- T g Glass transition temperature
- TMA thermomechanical analyzer
- ⁇ 50-300 Thermal expansion coefficient from 50 ° C to 300 ° C
- Examples 1 to 22 are examples.
- the flaky glasses having the respective compositions shown in Examples 2 and 3 were weighed, mixed and melted in the same manner as described above, and then the melt was poured into a gap between twin rolls and rapidly cooled. Each flake was dry pulverized with an alumina ball mill for 1 hour to obtain each glass frit. Each glass frit had a mass average particle size of about 3 microns. 75 g of each obtained glass frit was kneaded with 25 g of an organic vehicle (10% by mass of ethyl cellulose dissolved in ⁇ -terpineol) to prepare a glass paste.
- an organic vehicle 10% by mass of ethyl cellulose dissolved in ⁇ -terpineol
- This glass paste is printed on a 10cm square and 0.55mm thick soda lime glass substrate surface-coated with a silica film, and uniformly printed in the center with a 9cm square size so that the film thickness after firing is 30 ⁇ m.
- the soda lime glass used has a thermal expansion coefficient ( ⁇ 50-300 ) from 50 ° C. to 300 ° C. of 83 ⁇ 10 ⁇ 7 / K.
- the glass for the scattering layer of the organic LED element of the present invention is suitable as a scattering layer for the organic LED element because it has good adhesion to the substrate and does not cause problems such as warping and cracking. I understand that.
- soda lime glass manufactured by Asahi Glass Co., Ltd. was used as the glass substrate.
- the scattering layer was produced as follows. First, powder raw materials were prepared so that the glass composition was as shown in Table 5.
- the prepared powder raw material was dissolved in an electric furnace at 1050 ° C. for 90 minutes, held at 950 ° C. for 60 minutes, and then cast into a roll to obtain glass flakes.
- This glass has a glass transition temperature of 475 ° C., a yield point of 525 ° C., and a thermal expansion coefficient of 72 ⁇ 10 ⁇ 7 (1 / ° C.) (average value of 50 to 300 ° C.).
- the measurement was performed by a thermal expansion method using a thermal analyzer (manufactured by Bruker, trade name: TD5000SA) at a heating rate of 5 ° C./min.
- the refractive index nF at the F line (486.13 nm) is 2.00
- the refractive index nd at the d line (587.56 nm) is 1.98
- the refractive index nC at the C line (656.27 nm) is 1. .97.
- the measurement was performed with a refractometer (trade name: KPR-2000, manufactured by Kalnew Optical Industry Co., Ltd.).
- the prepared flakes were pulverized with a zirconia planetary mill for 2 hours and then sieved to obtain glass powder.
- the particle size distribution at this time was D50 of 2.15 ⁇ m, D10 of 0.50 ⁇ m, and D90 of 9.72 ⁇ m.
- 35 g of the obtained glass powder was kneaded with 13.1 g of an organic vehicle (ethyl cellulose dissolved in ⁇ -terpineol or the like) to prepare a glass paste.
- This glass paste was uniformly printed on the above-mentioned glass substrate so as to have a circular shape with a diameter of 10 mm and a film thickness after firing of 14 ⁇ m.
- haze measurement and surface waviness measurement were performed.
- a haze computer (trade name: HZ-2) manufactured by Suga Test Instruments Co., Ltd. was used, and a single glass substrate was used as a reference sample. That is, the total light transmittance is 100 and the haze is 0 when a single glass substrate is measured. As a result of measurement, the total light transmittance was 79, and the haze value was 52.
- the apparatus uses a surface roughness measuring machine manufactured by Kosaka Laboratory Ltd. (table name: Surfcorder ET4000A), the evaluation length is 5.0 mm, the cutoff wavelength is 2.5 mm, and the measurement speed is 0.1 mm / The roughness was measured with s. As a result, the arithmetic average roughness Ra was 0.55 ⁇ m, and the arithmetic average wavelength ⁇ a was 193 ⁇ m. These numerical values are based on the ISO 4287-1997 standard.
- ITO having a thickness of 150 nm was formed by DC magnetron sputtering as a translucent electrode. At the time of sputtering, a film is formed in a desired shape using a mask.
- the refractive index of ITO and the refractive index of the glass for scattering layers described above are shown in FIG. In the figure, the vertical axis represents the refractive index, and the horizontal axis represents the wavelength (unit: nm).
- ⁇ -NPD N, N′-diphenyl-N, N′-bis (l-naphthyl) -l, l′ biphenyl-4,4 ′′ diamine: CAS No. 123847 was used using a vacuum deposition apparatus. -85-4) was deposited to 100 nm, Alq3 (tris8-hydroxyquinoline aluminum: CAS No. 2085-33-8) to 60 nm, LiF to 0.5 nm, and Al to 80 nm.
- ⁇ -NPD and Alq3 form a circular pattern having a diameter of 12 mm using a mask, and LiF and Al form a pattern using a mask having a 2 mm square region on the ITO pattern through the organic film.
- the element substrate was completed.
- a glass substrate (PD200 manufactured by Asahi Glass Co., Ltd.) prepared separately was subjected to sand blasting to partially form a recess to create a counter substrate.
- Photosensitive epoxy resin was applied to the bank around the recess for sealing the periphery.
- the element substrate and the counter substrate are placed in a glove box in a nitrogen atmosphere, and a water catching material containing CaO is attached to the concave portion of the counter substrate, and then the element substrate and the counter substrate are bonded together and irradiated with ultraviolet rays. Then, the peripheral sealing resin was cured to complete the organic EL element.
- FIG. 4 and FIG. 5 show how the element emits light.
- FIG. 4 shows an element having a scattering layer
- FIG. 5 shows an element without a scattering layer
- 400 represents a scattering layer
- 410 represents an organic layer
- 420 represents an ITO pattern
- 430 represents an Al pattern.
- light emission is confirmed only from the approximately 2 mm square region formed by the crossing of the ITO pattern and the Al pattern.
- the element fabricated on the scattering layer not only the above approximately 2 mm square region. It can be seen that light is also extracted from the surrounding scattering layer forming portion into the atmosphere.
- FIG. 6 shows current-voltage characteristics of an element with and without a scattering layer.
- the vertical axis represents voltage (unit: V)
- the horizontal axis represents current (unit: mA).
- the current luminous flux characteristics are shown in FIG.
- the vertical axis indicates the luminous flux (unit: lm)
- the horizontal axis indicates the current (unit: mA).
- the amount of light flux is proportional to the current regardless of the presence or absence of the scattering layer. Furthermore, it was confirmed that the element having the scattering layer had a 51% increase in the luminous flux compared to the element having no scattering layer. As shown in FIG. 3, since the refractive index of the scattering layer is higher than the refractive index of ITO, which is a translucent electrode, at the emission wavelength of Alq3 (470 nm to 700 nm), the EL emission light of Alq3 is scattered with ITO. Suppressing total reflection at the interface of the layers, indicating that light is efficiently extracted into the atmosphere.
- the angle dependency of light emission was evaluated.
- a color luminance meter (trade name: BM-7A) manufactured by Topcon Technohouse Co., Ltd. was used, and as shown in FIG.
- the angle dependence of the luminescent color was measured.
- 800 indicates an evaluation element
- 810 indicates a spectrometer.
- a current of 1 mA is applied to the element to light it.
- the angle is defined as a measurement angle ⁇ [°], which is an angle formed between the normal direction of the element and the direction from the element toward the luminance meter. That is, the state where the luminance meter is installed in front of the element is 0 °.
- the luminance data obtained from the measurement is shown in FIG.
- the vertical axis represents luminance (unit: cd / m 2 ), and the horizontal axis represents angle (unit: °). Further, chromaticity data obtained from the measurement is shown in FIG. In the figure, the vertical axis represents V ′ and the horizontal axis represents U ′.
- the CIE1976UCS color system is used to calculate the chromaticity coordinates.
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Abstract
Description
ここで、有機LED素子も、有機LED素子の外部に取り出せる光の量は、発光光の20%足らずになっているのが現状である。
そこで、有機LED素子内にガラスからなる散乱層を設け、光の取り出し効率を向上させることを記載した文献がある(特許文献1)。
なお、近年、酸化鉛を含むガラスの溶解では、環境汚染が重大な問題となっている。従って、ガラスには酸化鉛を含まないことが要求されている。 The organic LED element has an organic layer. And there exists a bottom emission type which takes out the light produced | generated by the organic layer from a transparent substrate.
Here, the amount of light that can be extracted outside the organic LED element is also less than 20% of the emitted light.
Therefore, there is a document describing that a scattering layer made of glass is provided in an organic LED element to improve light extraction efficiency (Patent Document 1).
In recent years, environmental pollution has become a serious problem in melting glass containing lead oxide. Accordingly, the glass is required not to contain lead oxide.
本発明の一態様の有機LED素子は、透明基板と、透明基板上に設けられる第1の電極と、第1の電極上に設けられる有機層と、有機層上に設けられる第2の電極とを備え、更に、酸化物基準のモル%表示で、P2O5:15~30%と、Bi2O3:5~25%と、Nb2O5:5~27%と、ZnO:10~35%とを含有し、Li2OとNa2OとK2Oとからなるアルカリ金属酸化物の含有量が合量で5質量%以下である散乱層を有することを特徴とする。 The scattering layer glass of the organic LED element of one embodiment of the present invention is expressed in terms of mol% based on oxide, P 2 O 5 : 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27% and ZnO: 15 to 35%, and the total content of alkali metal oxides composed of Li 2 O, Na 2 O, and K 2 O is 5% by mass or less It is characterized by that.
An organic LED element of one embodiment of the present invention includes a transparent substrate, a first electrode provided on the transparent substrate, an organic layer provided on the first electrode, and a second electrode provided on the organic layer. Furthermore, in terms of mol% on the oxide basis, P 2 O 5 : 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27%, ZnO: 10 It is characterized by having a scattering layer containing ˜35% and containing a total amount of alkali metal oxides composed of Li 2 O, Na 2 O and K 2 O of 5% by mass or less.
初めに、図面を用いて、本発明の有機LED素子について説明する。
図1は、本発明の第1の有機LED素子の断面図である。本発明の第1の有機LED素子は、ボトムエミッションタイプの有機LED素子である。本発明の第1の有機LED素子は、透明基板110と、透明基板110上に形成された散乱層120と、散乱層120上に形成された第1の電極130と、第1の電極130上に形成された有機層140と、有機層140上に形成された第2の電極150とを有する。本発明の第1の有機LED素子において、第1の電極130は透明電極(陽極)であり、第2の電極150は反射電極(陰極)である。第1の電極130は、有機層140から発光された光を散乱層120へ伝えるための透明性を有する。一方、第2の電極150は、有機層140から発光された光を反射して有機層140へ戻すための反射性を有する。 (Organic LED element)
First, the organic LED element of the present invention will be described with reference to the drawings.
FIG. 1 is a cross-sectional view of a first organic LED element of the present invention. The first organic LED element of the present invention is a bottom emission type organic LED element. The first organic LED element of the present invention includes a
透明基板110の形成に用いられる透光性の基板としては、主としてガラス基板など、可視光に対する透過率が高い材料が用いられる。透過率の高い材料は、具体的には、ガラス基板のほかにはプラスチック基板が用いられる。ガラス基板の材料としては、アルカリガラス、無アルカリガラスまたは石英ガラスなどの無機ガラスがある。ガラス成分の拡散を防止するために、ガラス基板の表面にシリカ膜等がコートされていてもかまわない。また、プラスチック基板の材料としては、ポリエステル、ポリカーボネート、ポリエーテル、ポリスルホン、ポリエーテルスルホン、ポリビニルアルコールならびにポリフッ化ビニリデン及びポリフッ化ビニルなどのフッ素含有ポリマーがある。なお、基板を水分が透過するのを防止するために、プラスチック基板にバリア性をもたせる構成としても良い。透明基板の厚さは、ガラスの場合0.1mm~2.0mmが好ましい。但し、あまり薄いと強度が低下するので、0.5mm~1.0mmであることが特に好ましい。 (Transparent substrate)
As the light-transmitting substrate used for forming the
散乱層120は、塗布などの方法で基板上にガラス粉末を形成し、所望の温度で焼成することで形成され、第1の屈折率を有するベース材121と、ベース材121中に分散された、ベース材121と異なる第2の屈折率を有する複数の散乱物質122とを備える。複数の散乱物質122は、散乱層内部から最表面にむかって、散乱層中の散乱物質の層内分布が、小さくなっている。そして、散乱層をガラスで構成することにより、優れた散乱特性を有しつつも表面の平滑性を維持することができ、発光デバイスなどの光出射面側に用いることで極めて高効率の光取り出しを実現することができる。 (Scattering layer)
The
ベース材に特定の透過率スペクトルを持たせることにより、発光の色味を変化させることもできる。着色剤としては、遷移金属酸化物、希土類金属酸化物、金属コロイドなどの公知のものを、単独であるいは組み合わせて使うことができる。
ここで、一般的に、バックライトや照明用途では、白色発光させることが必要である。白色化は、赤、青、緑を空間的に塗り分ける方法(塗り分け法)、異なる発光色を有する発光層を積層する方法(積層法)、青色発光した光を空間的に分離して設けた色変換材料で色変換する方法(色変換法)が知られている。バックライトや照明用途では、均一に白色を得ればよいので、積層法が一般的である。積層する発光層は加色混合で白になるような組み合わせを用いる、例えば、青緑層とオレンジ層を積層する場合や、赤、青、緑を積層する場合がある。特に、照明用途では照射面での色再現性が重要で、可視光領域に必要な発光スペクトルを有していることが望ましい。青緑層とオレンジ層を積層する場合には、緑色の発光強度が低いため、緑を多く含んだものを照明すると、色再現性が悪くなってしまう。積層法は、空間的に色配置を変える必要がないというメリットがある一方で、以下2つの課題を抱えている。1つ目の問題は有機層の膜厚が薄いことから、取り出された発光光は干渉の影響を受ける。したがって、見る角度によって、色味が変化することになる。白色の場合には、人間の目の色味に対する感度が高いため、このような現象は問題になることがある。2つ目の問題は発光している間に、キャリアバランスがずれて、各色での発光輝度が変わり、色味が変わってしまうことである。 In order to obtain the maximum refractive index difference, it is desirable that the base material has a high refractive index glass and the scattering material has a gaseous object, that is, a bubble.
By giving the base material a specific transmittance spectrum, the color of light emission can be changed. As the colorant, known ones such as transition metal oxides, rare earth metal oxides and metal colloids can be used alone or in combination.
Here, in general, it is necessary to emit white light in a backlight or lighting application. Whitening is a method of spatially painting red, blue, and green (painting method), a method of laminating light emitting layers having different emission colors (lamination method), and providing blue light that is separated spatially. A method (color conversion method) for performing color conversion with a color conversion material is known. In backlight and lighting applications, a white layer can be obtained uniformly, so a lamination method is common. The light emitting layer to be stacked uses a combination that turns white by additive color mixing. For example, a blue-green layer and an orange layer may be stacked, or red, blue, and green may be stacked. In particular, for lighting applications, color reproducibility on the irradiated surface is important, and it is desirable to have a necessary emission spectrum in the visible light region. When the blue-green layer and the orange layer are laminated, the green light emission intensity is low, and therefore, when a light containing a lot of green is illuminated, the color reproducibility is deteriorated. While the lamination method has an advantage that it is not necessary to spatially change the color arrangement, it has the following two problems. The first problem is that since the organic layer is thin, the extracted emitted light is affected by interference. Therefore, the color changes depending on the viewing angle. In the case of white, such a phenomenon may be a problem because the sensitivity to the color of human eyes is high. The second problem is that the carrier balance is shifted while the light is emitted, the light emission luminance of each color is changed, and the color is changed.
第1の電極(陽極)は、有機層140で発生した光を外部に取り出すために、80%以上の透光性が要求される。また、多くの正孔を注入するため、仕事関数が高いものが要求される。具体的には、ITO(Indium Tin Oxide)、SnO2、ZnO、IZO(Indium Zinc Oxide)、AZO(ZnO-Al2O3:アルミニウムがドーピングされた亜鉛酸化物)、GZO(ZnO-Ga2O3:ガリウムがドーピングされた亜鉛酸化物)、NbドープTiO2、TaドープTiO2などの材料が用いられる。陽極の厚さは、100nm以上が好ましい。なお、陽極130の屈折率は、1.9~2.2である。ここで、キャリア濃度を増加させると、ITOの屈折率を低下させることができる。市販されているITOは、SnO2が10wt%が標準となっているが、これより、Sn濃度を増やすことで、ITOの屈折率を下げることができる。但し、Sn濃度増加により、キャリア濃度は増加するが、移動度及び透過率の低下があるため、これらのバランスをとって、Sn量を決める必要がある。 (First electrode)
The first electrode (anode) is required to have a translucency of 80% or more in order to extract light generated in the
有機層140は、発光機能を有する層であり、正孔注入層と、正孔輸送層と、発光層と、電子輸送層と、電子注入層とにより構成される。有機層140の屈折率は、1.7~1.8である。
正孔注入層は、陽極からの正孔注入障壁を低くするために、イオン化ポテンシャルの差が小さいものが要求される。正孔注入層における電極界面からの電荷の注入効率の向上は、素子の駆動電圧を下げるとともに、電荷の注入効率を高める。高分子では、ポリスチレンスルフォン酸(PSS)がドープされたポリエチレンジオキシチオフェン(PEDOT:PSS)、低分子ではフタロシアニン系の銅フタロシアニン(CuPc)が広く用いられる。
正孔輸送層は、正孔注入層から注入された正孔を発光層に輸送する役割をする。適切なイオン化ポテンシャルと正孔移動度を有することが必要である。正孔輸送層は、具体的には、トリフェニルアミン誘導体、N,N’-ビス(1-ナフチル)-N,N’-ジフェニル-1,1’-ビフェニル-4,4’-ジアミン(NPD)、N,N’-ジフェニル-N,N’-ビス[N-フェニル-N-(2-ナフチル)-4’-アミノビフェニル-4-イル]-1,1’-ビフェニル-4,4’-ジアミン(NPTE)、1,1-ビス[(ジ-4-トリルアミノ)フェニル]シクロヘキサン(HTM2)及びN,N’-ジフェニル-N,N’-ビス(3-メチルフェニル)-1,1’-ジフェニル-4,4’-ジアミン(TPD)などが用いられる。正孔輸送層の厚さは、10nm~150nmが好ましい。厚さは薄ければ薄いほど低電圧化できるが、電極間短絡の問題から10nm~150nmであることが特に好ましい。 (Organic layer)
The
The hole injection layer is required to have a small difference in ionization potential in order to lower the hole injection barrier from the anode. Improvement of the charge injection efficiency from the electrode interface in the hole injection layer lowers the drive voltage of the device and increases the charge injection efficiency. Polyethylene dioxythiophene (PEDOT: PSS) doped with polystyrene sulfonic acid (PSS) is widely used for polymers, and phthalocyanine-based copper phthalocyanine (CuPc) is widely used for low molecules.
The hole transport layer serves to transport holes injected from the hole injection layer to the light emitting layer. It is necessary to have an appropriate ionization potential and hole mobility. Specifically, the hole transport layer may be a triphenylamine derivative, N, N′-bis (1-naphthyl) -N, N′-diphenyl-1,1′-biphenyl-4,4′-diamine (NPD ), N, N′-diphenyl-N, N′-bis [N-phenyl-N- (2-naphthyl) -4′-aminobiphenyl-4-yl] -1,1′-biphenyl-4,4 ′ -Diamine (NPTE), 1,1-bis [(di-4-tolylamino) phenyl] cyclohexane (HTM2) and N, N'-diphenyl-N, N'-bis (3-methylphenyl) -1,1 '-Diphenyl-4,4'-diamine (TPD) or the like is used. The thickness of the hole transport layer is preferably 10 nm to 150 nm. The thinner the thickness is, the lower the voltage can be. However, the thickness is particularly preferably 10 nm to 150 nm from the problem of short circuit between electrodes.
電子注入層は、電子の注入効率を高めるものが要求される。電子注入層は、具体的には、陰極界面にリチウム(Li)、セシウム(Cs)等のアルカリ金属をドープした層を設ける。 The electron transport layer serves to transport electrons injected from the electrode. Specifically, the electron transport layer is formed of a quinolinol aluminum complex (Alq 3 ), an oxadiazole derivative (for example, 2,5-bis (1-naphthyl) -1,3,4-oxadiazole (BND) and 2 -(4-t-butylphenyl) -5- (4-biphenyl) -1,3,4-oxadiazole (PBD) and the like), triazole derivatives, bathophenanthroline derivatives, silole derivatives and the like are used.
The electron injection layer is required to increase the electron injection efficiency. Specifically, the electron injection layer is provided with a layer doped with an alkali metal such as lithium (Li) or cesium (Cs) at the cathode interface.
第2の電極としての反射性電極(陰極)は、仕事関数の小さな金属またはその合金が用いられる。陰極は、具体的には、アルカリ金属、アルカリ土類金属及び周期表第3族の金属などが挙げられる。このうち、安価で化学的安定性の良い材料であることから、アルミニウム(Al)、マグネシウム(Mg)、銀(Ag)またはこれらの合金などが好ましく用いられる。また、Al、MgAgの共蒸着膜、LiFまたはLi2Oの薄膜蒸着膜の上にAlを蒸着した積層電極等が用いられる。また、高分子系では、カルシウム(Ca)またはバリウム(Ba)とアルミニウム(Al)の積層等が用いられる。なお、反射性電極を陽極としても良いことは言うまでもない。
ここで、第2の電極は、両面エミッションタイプの第2の有機LED素子で用いられる場合、反射性ではなく、透光性が要求される。そのため、そのときの構成及び特性は、第1の電極と同じものが良い。 (Second electrode)
For the reflective electrode (cathode) as the second electrode, a metal having a small work function or an alloy thereof is used. Specific examples of the cathode include alkali metals, alkaline earth metals, metals of
Here, when the second electrode is used in the second organic LED element of the double-sided emission type, it is not reflective but requires translucency. Therefore, the configuration and characteristics at that time are preferably the same as those of the first electrode.
次に、本発明の有機LED素子の散乱層用ガラスについて詳細に説明する。
散乱層用ガラスの屈折率は、前記のとおり透光性電極材料の屈折率と同等または若しくは高い方が好ましいため、できるだけ高いことが望まれる。また、散乱層用ガラスのガラス転移温度は、ガラス粉末を焼成して軟化させ散乱層を形成する際に、基板の熱変形を防ぐため、できるだけ低いことが望まれる。また、散乱層用ガラスの熱膨張係数は、散乱層を形成する際に基板との間に応力が発生して割れたり反ったりする現象を防ぐため、基板の熱膨張係数と近いか若干低い必要がある。一般的には高屈折率と低転移温度を有するガラスの熱膨張係数は基板の熱膨張係数よりもきわめて大きいため、散乱層用ガラスの熱膨張係数はできるだけ低いことが望まれる。反りや割れは、散乱層上に透光性電極層を形成する際に大きな障害となる。 (Glass for scattering layer)
Next, the scattering layer glass of the organic LED element of the present invention will be described in detail.
Since the refractive index of the glass for a scattering layer is preferably equal to or higher than the refractive index of the translucent electrode material as described above, it is desirable that it be as high as possible. The glass transition temperature of the glass for the scattering layer is desirably as low as possible in order to prevent thermal deformation of the substrate when the glass powder is fired and softened to form the scattering layer. In addition, the thermal expansion coefficient of the glass for the scattering layer must be close to or slightly lower than the thermal expansion coefficient of the substrate in order to prevent the phenomenon of cracking or warping due to stress generated between the scattering layer and the substrate. There is. In general, the glass having a high refractive index and a low transition temperature has a coefficient of thermal expansion that is much larger than the coefficient of thermal expansion of the substrate. Therefore, it is desirable that the coefficient of thermal expansion of the glass for the scattering layer be as low as possible. Warpage and cracking become a major obstacle when forming a translucent electrode layer on a scattering layer.
P2O5は、ガラスの骨格となる網目構造を形成し、ガラスを安定化させる成分であり、必須である。P2O5が15モル%未満では、失透しやすくなる。19モル%以上が好ましくは、20モル%以上がより好ましい。一方、30モル%を超えると、高屈折率を得ることが難しくなる。28モル%以下が好ましく、26モル%以下がより好ましい。
Bi2O3は、高屈折率を付与し、ガラスの安定性を高める成分であり、必須である。5%未満では、その効果が不十分となる。10モル%以上が好ましく、13モル%以上がより好ましい。一方、25モル%を超えると、熱膨張係数を高くし、着色を大きくしやすくなる。23モル%以下が好ましく、20モル%以下がより好ましい。
Nb2O5は、高屈折率を付与するとともに熱膨張係数を下げる成分であり、必須である。5モル%未満では、その効果が不十分となる。7モル%以上が好ましく、10モル%以上がより好ましい。一方、27モル%を超えると、ガラス転移温度を高くし、失透しやすくなる。20モル%以下が好ましく、18モル%以下がより好ましい。
ZnOは、熱膨張係数の過度の上昇を抑えながらガラス転移温度を大きく下げるとともに屈折率を高くする成分であり、必須である。10モル%未満ではその効果が不十分となる。16モル%以上が好ましく、18モル%以上がより好ましい。一方、35モル%を超えると、ガラスの失透傾向が強まる。30モル%以下が好ましく、27モル%以下がより好ましい。なお、モル%表記とは必ずしも一対一に対応しないが、質量%で表すと、7質量%以上が好ましい。
Li2O、Na2O及びK2Oからなるアルカリ金属酸化物は、熱膨張係数を大きくするおそれがある。そのため、実質的に含有しない(含有量がほぼ零である)ことが好ましい。しかし、ガラスの耐失透性を付与するとともにガラス転移温度を下げる効果を有するため、7モル%まで含有してもよい。 In terms of mol% based on the oxide of the present invention, P 2 O 5 : 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27%, ZnO: 10 to 35 %, And the total content of alkali metal oxides composed of Li 2 O, Na 2 O, and K 2 O is 5% by mass or less.
P 2 O 5 is a component that forms a network structure serving as a skeleton of the glass and stabilizes the glass, and is essential. When P 2 O 5 is less than 15 mol%, devitrification is likely to occur. 19 mol% or more is preferable, and 20 mol% or more is more preferable. On the other hand, when it exceeds 30 mol%, it is difficult to obtain a high refractive index. 28 mol% or less is preferable and 26 mol% or less is more preferable.
Bi 2 O 3 is a component that imparts a high refractive index and increases the stability of the glass, and is essential. If it is less than 5%, the effect becomes insufficient. 10 mol% or more is preferable and 13 mol% or more is more preferable. On the other hand, when it exceeds 25 mol%, the thermal expansion coefficient is increased, and the coloring is easily increased. 23 mol% or less is preferable and 20 mol% or less is more preferable.
Nb 2 O 5 is a component that imparts a high refractive index and lowers the thermal expansion coefficient, and is essential. If it is less than 5 mol%, the effect becomes insufficient. 7 mol% or more is preferable and 10 mol% or more is more preferable. On the other hand, when it exceeds 27 mol%, the glass transition temperature is increased and devitrification is likely to occur. 20 mol% or less is preferable and 18 mol% or less is more preferable.
ZnO is a component that greatly lowers the glass transition temperature and increases the refractive index while suppressing an excessive increase in the thermal expansion coefficient, and is essential. If it is less than 10 mol%, the effect becomes insufficient. 16 mol% or more is preferable and 18 mol% or more is more preferable. On the other hand, if it exceeds 35 mol%, the devitrification tendency of the glass increases. 30 mol% or less is preferable and 27 mol% or less is more preferable. In addition, although it does not necessarily respond | correspond one-to-one with mol% notation, when expressed in mass%, 7 mass% or more is preferable.
Alkali metal oxides composed of Li 2 O, Na 2 O and K 2 O may increase the thermal expansion coefficient. Therefore, it is preferable not to contain substantially (content is substantially zero). However, since it has the effect of giving the glass devitrification resistance and lowering the glass transition temperature, it may be contained up to 7 mol%.
また、Na2O及びK2Oは、Li2Oに比して特に熱膨張係数を大きくしてしまうため、アルカリ金属酸化物を含有させる場合、Na2OとK2Oを実質的に含まず(含有量がほぼ零である)、Li2Oのみを用いることが好ましい。
TiO2は、ガラス転移温度が上昇するとともに失透しやすくなる。そのため、TiO2は、実質的に含まない(含有量がほぼ零である)ことが好ましい。しかし、高屈折率を付与する効果を有するため、8モル%まで含有してもよい。
B2O3は必須ではないが、ガラスの溶解性を向上させる効果を有する。そのため、17モル%まで含有してもよい。しかし、17モル%を超えると失透や分相が生じやすくなるとともに高屈折率を得ることが難しくなる。
WO3は必須ではないが、熱膨張係数とガラス転移温度を大きく変化させずに高屈折率を付与する効果を有する。そのため、20モル%まで含有してもよい。しかし、20モル%を超えると着色が大きくなるとともに、失透しやすくなる。
TeO2は必須ではないが、熱膨張係数の過度の上昇を抑えながらガラス転移温度を下げる効果を有する。そのため、7モル%まで含有してもよい。しかし、高価であり、また白金坩堝を侵食する恐れがあるため、多量に使用しないほうが好ましい。
GeO2は必須ではないが、高屈折率を付与する効果を有する。そのため、7モル%まで含有してもよい。しかし、高価であるため多量に使用しないほうが好ましい。
Sb2O3は必須ではないが、清澄剤として有効であるばかりでなく、着色を抑制する効果も有る。そのため、2モル%まで含有してもよい。
アルカリ土類金属酸化物(MgO、CaO、SrO、BaO)は必須ではないが、ガラスの安定性を向上させる効果を有する。そのため、10モル%まで含有してもよい。しかし、10モル%を超えて含有すると、屈折率を低下させるとともに熱膨張係数を大きくしてしまう。
なお、実質的に含有しないとは、積極的に含有しないということであり、他の成分由来による不純物として混入される場合を含むものとする Here, the alkali metal may move when an electric field is applied in a humid state, and may destroy the terminal of the organic LED element. Therefore, the total amount of the alkali metal oxide is preferably 5% by mass or less, more preferably 2% by mass or less, and particularly preferably substantially not contained (the content is substantially zero).
Further, Na 2 O and K 2 O, since the result in particularly large thermal expansion coefficient compared to Li 2 O, if the inclusion of alkali metal oxides, substantially free of Na 2 O and K 2 O (Content is almost zero), it is preferable to use only Li 2 O.
TiO 2 tends to devitrify as the glass transition temperature rises. Therefore, it is preferable that TiO 2 is not substantially contained (the content is substantially zero). However, since it has an effect of imparting a high refractive index, it may be contained up to 8 mol%.
B 2 O 3 is not essential, but has an effect of improving the solubility of the glass. Therefore, you may contain to 17 mol%. However, if it exceeds 17 mol%, devitrification and phase separation are likely to occur, and it becomes difficult to obtain a high refractive index.
WO 3 is not essential, but has the effect of imparting a high refractive index without significantly changing the thermal expansion coefficient and glass transition temperature. Therefore, you may contain to 20 mol%. However, when it exceeds 20 mol%, coloring increases and devitrification easily occurs.
TeO 2 is not essential, but has an effect of lowering the glass transition temperature while suppressing an excessive increase in the thermal expansion coefficient. Therefore, you may contain to 7 mol%. However, it is expensive and may erode the platinum crucible, so it is preferable not to use a large amount.
GeO 2 is not essential, but has an effect of imparting a high refractive index. Therefore, you may contain to 7 mol%. However, since it is expensive, it is preferable not to use a large amount.
Sb 2 O 3 is not essential, but it is not only effective as a clarifying agent but also has an effect of suppressing coloring. Therefore, you may contain to 2 mol%.
Alkaline earth metal oxides (MgO, CaO, SrO, BaO) are not essential, but have the effect of improving the stability of the glass. Therefore, you may contain to 10 mol%. However, if the content exceeds 10 mol%, the refractive index is lowered and the thermal expansion coefficient is increased.
In addition, it does not contain substantially when it does not contain substantially, and includes the case where it mixes as an impurity by other ingredients origin.
なお、本発明のガラスは、酸化鉛を実質的に含有しないため、環境汚染を引き起こす可能性が低い。
本発明のガラスは、酸化物、リン酸塩、メタリン酸塩、炭酸塩、硝酸塩、水酸化物等の原料を使用し、それらを所定の組成になるよう秤取し、混合した後、白金等の坩堝を用いて950~1500℃の温度で溶解し、鋳型に鋳込むか双ロールの隙間に注いで急冷することによって得ることができる。また、徐冷して歪みを取り除くこともある。以上の方法によって作製したガラスを粉末の形態で用いる。ガラス粉末は、ガラスを、乳鉢、ボールミル、ジェットミル等により粉砕し、必要に応じて分級することによって得られる。ガラス粉末の質量平均粒径は、典型的には、0.5~10ミクロンである。界面活性剤やシランカップリング剤によってガラス粉末の表面を改質しても良い。
このガラスフリットを、必要に応じて溶剤やバインダーなどと混練後、透明基板上に塗布し、ガラスフリットのガラス転移温度より60℃程度以上高い温度で焼成してガラスフリットを軟化させ、室温まで冷却することによって、散乱層付き透明基板が得られる。溶剤としては、α-テルピネオール、ブチルカルビトールアセテート、フタル酸エステル、2,2,4-トリメチル-1,3-ペンタンジオールモノイソブチレート等が、バインダーとしては、エチルセルロース、アクリル樹脂、スチレン樹脂、フェノール樹脂、ブチラール樹脂等が、それぞれ例示される。なお、本発明の目的を損なわない範囲で溶剤またはバインダー以外の成分を含有してもよい。なお、バインダーを用いる場合は、ガラスフリットを軟化させる前に、ガラス転移温度よりも低い温度で焼成してバインダーを気化させる工程を含むことが好ましい。 The glass of the present invention is SiO 2 , Al 2 O 3 , La 2 O 3 , Y 2 O 3 , Gd 2 O 3 , ZrO 2 , Ta 2 O 3 , Cs 2 O, as long as the effects of the invention are not lost. Transition metal oxides and the like can also be contained. Their total content is preferably less than 5 mol%, more preferably less than 3 mol%, and particularly preferably substantially no content (the content is almost zero).
In addition, since the glass of this invention does not contain lead oxide substantially, possibility of causing environmental pollution is low.
The glass of the present invention uses raw materials such as oxides, phosphates, metaphosphates, carbonates, nitrates, and hydroxides, weighs them so as to have a predetermined composition, mixes them, platinum, etc. It can be obtained by melting at a temperature of 950 to 1500 ° C. using a crucible and casting into a mold or pouring into a gap between twin rolls and quenching. Also, it may be gradually cooled to remove the distortion. The glass produced by the above method is used in the form of powder. The glass powder is obtained by pulverizing glass with a mortar, ball mill, jet mill or the like, and classifying it as necessary. The mass average particle size of the glass powder is typically 0.5 to 10 microns. The surface of the glass powder may be modified with a surfactant or a silane coupling agent.
This glass frit is kneaded with a solvent or a binder as necessary, and then applied onto a transparent substrate and fired at a temperature about 60 ° C. higher than the glass transition temperature of the glass frit to soften the glass frit and cool to room temperature. By doing so, a transparent substrate with a scattering layer is obtained. Examples of the solvent include α-terpineol, butyl carbitol acetate, phthalate ester, 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, and the binder includes ethyl cellulose, acrylic resin, styrene resin, Examples thereof include phenol resin and butyral resin. In addition, you may contain components other than a solvent or a binder in the range which does not impair the objective of this invention. In addition, when using a binder, before softening a glass frit, it is preferable to include the process of baking at a temperature lower than a glass transition temperature and vaporizing a binder.
得られたガラスについて、屈折率(nd)、ガラス転移温度(Tg)、50℃から300℃までの熱膨張係数(α50-300)を以下のようにして測定した。
(1)屈折率(nd)
ガラスを研磨した後、カルニュー社製精密屈折計KPR-2000によって、Vブロック法で測定した。
(2)ガラス転移温度(Tg)
ガラスを直径5mm長さ200mmの丸棒状に加工した後、ブルッカー・エイエックスエス社製熱機械分析装置(TMA)TD5000SAによって、昇温速度を5℃/minにして測定した。
(3)50℃から300℃までの熱膨張係数(α50-300)
ガラスを直径5mm長さ200mmの丸棒状に加工した後、ブルッカー・エイエックスエス社製熱機械分析装置(TMA)TD5000SAによって、昇温速度を5℃/minにして測定した。50℃に於けるガラス棒の長さをL50とし、300度におけるガラス棒の長さをL300としたとき、50℃から300℃までの熱膨張係数(α50-300)は、α50-300={(L300/L50)―1}/(300-50)によって求められる。 Tables 1 to 3 show the composition of the glass expressed in mol% in each example, the refractive index (n d ), the glass transition temperature (T g ), and the average thermal expansion coefficient from 50 ° C. to 300 ° C. ( α 50-300 ). In addition, the composition in terms of mass% converted based on the composition in terms of mol% is also shown. In any glass, oxides, metaphosphates or carbonates are used as raw materials for each component. After vitrification, the raw materials are weighed so as to have the composition shown in Table 1 and mixed sufficiently, and then a platinum crucible is used. After melting in a temperature range of 950 ° C. to 1350 ° C. in an electric furnace, it is cast into a carbon mold, the cast glass is cooled to a transition temperature, immediately put into an annealing furnace, and gradually cooled to room temperature. Got.
With respect to the obtained glass, the refractive index (n d ), glass transition temperature (T g ), and thermal expansion coefficient (α 50-300 ) from 50 ° C. to 300 ° C. were measured as follows.
(1) Refractive index (n d )
After the glass was polished, it was measured by a V-block method using a Kalun precision refractometer KPR-2000.
(2) Glass transition temperature (T g )
The glass was processed into a round bar shape having a diameter of 5 mm and a length of 200 mm, and then measured with a thermomechanical analyzer (TMA) TD5000SA manufactured by Bruker AXS Co., Ltd. at a heating rate of 5 ° C./min.
(3) Thermal expansion coefficient from 50 ° C to 300 ° C (α 50-300 )
The glass was processed into a round bar shape having a diameter of 5 mm and a length of 200 mm, and then measured with a thermomechanical analyzer (TMA) TD5000SA manufactured by Bruker AXS Co., Ltd. at a heating rate of 5 ° C./min. When the length of the glass rod at 50 ° C. is L 50 and the length of the glass rod at 300 ° is L 300 , the thermal expansion coefficient (α 50-300 ) from 50 ° C. to 300 ° C. is α 50 −300 = {(L 300 / L 50 ) −1} / (300−50)
まず、ガラス基板としては、旭硝子株式会社製ソーダライムガラスを用いた。散乱層は以下のように作製した。まずガラス組成が表5になるように粉末原料を調合した。 Next, a confirmation experiment for improving the light extraction efficiency will be described.
First, soda lime glass manufactured by Asahi Glass Co., Ltd. was used as the glass substrate. The scattering layer was produced as follows. First, powder raw materials were prepared so that the glass composition was as shown in Table 5.
ヘイズ測定には、スガ試験機社製ヘーズコンピュータ(商品名:HZ-2)を用い、基準サンプルとしてガラス基板単体を用いた。つまり、ガラス基板単体を測定したときに全光線透過率が100、ヘイズが0となるように構成される。こうして測定した結果、全光線透過率は79、ヘイズ値は52であった。 In order to evaluate the characteristics of the glass substrate with a scattering layer thus prepared, haze measurement and surface waviness measurement were performed.
For the haze measurement, a haze computer (trade name: HZ-2) manufactured by Suga Test Instruments Co., Ltd. was used, and a single glass substrate was used as a reference sample. That is, the total light transmittance is 100 and the haze is 0 when a single glass substrate is measured. As a result of measurement, the total light transmittance was 79, and the haze value was 52.
まず、全光束測定には、浜松ホトニクス社製EL特性測定機C9920-12を用いた。散乱層がある素子とない素子での電流電圧特性を図6に示す。なお、図中、縦軸は電圧(単位:V)を示し、横軸は電流(単位:mA)を示す。このように、ほぼ同程度の特性が得られており、散乱層上に形成した素子でも、大きなリーク電流が存在しないことが分かる。次に電流光束特性を図7に示す。なお、なお、図中、縦軸は光束(単位:lm)を示し、横軸は電流(単位:mA)を示す。このように散乱層の有無に関わらず、光束量が電流に比例している。さらに、散乱層がある素子は、散乱層がない素子と比較して、光束量が51%アップしていることが確認できた。これは、図3に示すように、散乱層の屈折率が、Alq3の発光波長(470nmから700nm)において透光性電極であるITOの屈折率より高いため、Alq3のEL発光光がITOと散乱層の界面で全反射するのを抑制し、効率よく光が大気中に取り出されていることを示している。 Thereafter, the optical characteristics of the element were evaluated.
First, an EL characteristic measuring machine C9920-12 manufactured by Hamamatsu Photonics was used for measuring the total luminous flux. FIG. 6 shows current-voltage characteristics of an element with and without a scattering layer. In the figure, the vertical axis represents voltage (unit: V), and the horizontal axis represents current (unit: mA). Thus, almost the same characteristics are obtained, and it can be seen that a large leak current does not exist even in the element formed on the scattering layer. Next, the current luminous flux characteristics are shown in FIG. In the figure, the vertical axis indicates the luminous flux (unit: lm), and the horizontal axis indicates the current (unit: mA). As described above, the amount of light flux is proportional to the current regardless of the presence or absence of the scattering layer. Furthermore, it was confirmed that the element having the scattering layer had a 51% increase in the luminous flux compared to the element having no scattering layer. As shown in FIG. 3, since the refractive index of the scattering layer is higher than the refractive index of ITO, which is a translucent electrode, at the emission wavelength of Alq3 (470 nm to 700 nm), the EL emission light of Alq3 is scattered with ITO. Suppressing total reflection at the interface of the layers, indicating that light is efficiently extracted into the atmosphere.
120 散乱層
130 第1の電極
140 有機層
150、210 第2の電極 110
Claims (10)
- 酸化物基準のモル%表示で、
P2O5 15~30%と、
Bi2O3 5~25%と、
Nb2O5 5~27%と、
ZnO 4~35%とを含有し、
Li2OとNa2OとK2Oとからなるアルカリ金属酸化物の含有量が合量で5質量%以下であることを特徴とする有機LED素子の散乱層用ガラス。 In mol% display based on oxide,
P 2 O 5 15-30%,
Bi 2 O 3 5-25%,
Nb 2 O 5 5 to 27%,
ZnO 4 to 35%,
A glass for a scattering layer of an organic LED element, wherein the total content of alkali metal oxides composed of Li 2 O, Na 2 O, and K 2 O is 5% by mass or less. - 前記アルカリ金属酸化物の含有量が合量で2質量%以下であることを特徴とする請求項1に記載の有機LED素子の散乱層用ガラス。 2. The glass for a scattering layer of an organic LED element according to claim 1, wherein the total content of the alkali metal oxide is 2% by mass or less.
- 前記アルカリ金属酸化物を実質的に含有しないことを特徴とする請求項1若しくは2に記載の有機LED素子の散乱層用ガラス。 The glass for a scattering layer of an organic LED element according to claim 1 or 2, wherein the glass does not substantially contain the alkali metal oxide.
- TiO2の含有量を実質的に含有しないことを特徴とする請求項1から3のいずれか一つに記載の有機LED素子の散乱層用ガラス。 The glass for a scattering layer of an organic LED element according to any one of claims 1 to 3, wherein the glass contains substantially no TiO 2 content.
- 酸化鉛の含有量を実質的に含有しないことを特徴とする請求項1から4のいずれか一つに記載の有機LED素子の散乱層用ガラス。 The glass for a scattering layer of an organic LED element according to any one of claims 1 to 4, which does not substantially contain a lead oxide content.
- 透明基板と、前記透明基板上に設けられる第1の電極と、前記第1の電極上に設けられる有機層と、前記有機層上に設けられる第2の電極とを備えた有機LED素子であって、
酸化物基準のモル%表示で、P2O5:15~30%と、Bi2O3:5~25%と、Nb2O5:5~27%と、ZnO:4~35%とを含有し、Li2OとNa2OとK2Oとからなるアルカリ金属酸化物の含有量が合量で5質量%以下である散乱層を有することを特徴とする有機LED素子。 An organic LED element comprising a transparent substrate, a first electrode provided on the transparent substrate, an organic layer provided on the first electrode, and a second electrode provided on the organic layer. And
P 2 O 5 : 15 to 30%, Bi 2 O 3 : 5 to 25%, Nb 2 O 5 : 5 to 27%, ZnO: 4 to 35% An organic LED element comprising a scattering layer containing and containing an alkali metal oxide composed of Li 2 O, Na 2 O, and K 2 O in a total amount of 5% by mass or less. - 前記散乱層は前記透明基板上に設けられることを特徴とする請求項6に記載の有機LED素子。 The organic LED element according to claim 6, wherein the scattering layer is provided on the transparent substrate.
- 前記散乱層は前記有機層上に設けられることを特徴とする請求項6に記載の有機LED素子。 The organic LED element according to claim 6, wherein the scattering layer is provided on the organic layer.
- 前記第1及び第2の電極は透明電極である請求項6から8のいずれか一つに記載の有機LED素子。 The organic LED element according to any one of claims 6 to 8, wherein the first and second electrodes are transparent electrodes.
- 照明に用いられる請求項6から9のいずれか一つに記載の有機LED素子。 10. The organic LED element according to any one of claims 6 to 9, which is used for illumination.
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US (1) | US8368064B2 (en) |
EP (1) | EP2383235B1 (en) |
JP (1) | JP5531967B2 (en) |
KR (1) | KR20110113177A (en) |
CN (1) | CN102292301B (en) |
TW (1) | TW201044665A (en) |
WO (1) | WO2010084922A1 (en) |
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Also Published As
Publication number | Publication date |
---|---|
KR20110113177A (en) | 2011-10-14 |
US20110278622A1 (en) | 2011-11-17 |
JP5531967B2 (en) | 2014-06-25 |
CN102292301A (en) | 2011-12-21 |
EP2383235B1 (en) | 2017-09-13 |
CN102292301B (en) | 2013-12-25 |
EP2383235A1 (en) | 2011-11-02 |
JPWO2010084922A1 (en) | 2012-07-19 |
US8368064B2 (en) | 2013-02-05 |
TW201044665A (en) | 2010-12-16 |
EP2383235A4 (en) | 2014-07-02 |
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